#------------------------------------------------------------------------------
#$Date: 2019-11-23 08:14:00 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232529 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/78/4347829.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4347829
loop_
_publ_author_name
'Hausmann, David'
'Feldmann, Claus'
_publ_section_title
;
 Bromine-rich Zinc Bromides: Zn6Br12(18-crown-6)2× (Br2)5,
 Zn4Br8(18-crown-6)2× (Br2)3, and Zn6Br12(18-crown-6)2×
 (Br2)2.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6141
_journal_page_last               6147
_journal_paper_doi               10.1021/acs.inorgchem.6b00663
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C12 H24 Br8 O6 Zn3'
_chemical_formula_weight         1099.70
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.32(3)
_cell_angle_beta                 91.43(3)
_cell_angle_gamma                106.82(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8990(18)
_cell_length_b                   11.163(2)
_cell_length_c                   14.937(3)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      1.93
_cell_volume                     1368.7(6)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10369
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    14.309
_exptl_absorpt_correction_T_max  0.2529
_exptl_absorpt_correction_T_min  0.0729
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.369
_refine_diff_density_min         -1.995
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0712P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                4129
_reflns_number_total             5251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00663_si_004.cif
_cod_data_source_block           '[Zn2Br3(18-crown-6)]2[Zn2Br6(Br2)2]'
_cod_original_cell_volume        1368.8(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4347829
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.75502(7) 0.14733(7) 0.20319(5) 0.03090(18) Uani 1 1 d .
Zn2 Zn 0.94889(8) 0.25399(8) -0.00545(5) 0.0362(2) Uani 1 1 d .
Zn3 Zn 0.52987(8) -0.39734(8) 0.43245(5) 0.0362(2) Uani 1 1 d .
Br1 Br 0.85827(8) 0.06643(7) 0.05957(5) 0.03929(18) Uani 1 1 d .
Br2 Br 1.21161(8) 0.36355(8) 0.04359(6) 0.0510(2) Uani 1 1 d .
Br3 Br 0.85005(7) 0.20078(7) -0.16010(5) 0.04235(19) Uani 1 1 d .
Br4 Br 0.44714(8) -0.46032(8) 0.27465(5) 0.0473(2) Uani 1 1 d .
Br5 Br 0.66118(8) -0.17286(7) 0.49377(5) 0.04372(19) Uani 1 1 d .
Br6 Br 0.68955(7) -0.52584(7) 0.47564(5) 0.03794(18) Uani 1 1 d .
Br7 Br 0.99144(9) -0.19635(8) 0.45121(6) 0.0496(2) Uani 1 1 d .
Br8 Br 1.23893(12) -0.21242(13) 0.42893(11) 0.0891(4) Uani 1 1 d .
O1 O 0.8734(5) 0.3458(5) 0.2495(3) 0.0366(10) Uani 1 1 d .
O2 O 0.9430(5) 0.1620(5) 0.2988(3) 0.0413(11) Uani 1 1 d .
O3 O 0.7153(5) -0.0517(5) 0.2202(3) 0.0393(11) Uani 1 1 d .
O4 O 0.5771(5) 0.1297(5) 0.2887(3) 0.0377(10) Uani 1 1 d .
O5 O 0.5645(5) 0.1871(5) 0.1302(3) 0.0397(11) Uani 1 1 d .
O6 O 0.8121(5) 0.3617(5) 0.0653(3) 0.0369(10) Uani 1 1 d .
C1 C 0.6476(7) 0.3369(7) 0.0365(5) 0.0400(15) Uani 1 1 d .
H1A H 0.6361 0.3479 -0.0268 0.048 Uiso 1 1 calc R
H1B H 0.6059 0.4000 0.0791 0.048 Uiso 1 1 calc R
C2 C 0.8785(8) 0.4759(7) 0.1415(5) 0.0405(15) Uani 1 1 d .
H2A H 0.8451 0.5485 0.1301 0.049 Uiso 1 1 calc R
H2B H 0.9951 0.5010 0.1449 0.049 Uiso 1 1 calc R
C3 C 0.5561(7) 0.2026(7) 0.0371(4) 0.0366(15) Uani 1 1 d .
H3A H 0.4445 0.1845 0.0138 0.044 Uiso 1 1 calc R
H3B H 0.5991 0.1396 -0.0046 0.044 Uiso 1 1 calc R
C4 C 0.8273(8) 0.4531(7) 0.2314(5) 0.0369(14) Uani 1 1 d .
H4A H 0.8760 0.5326 0.2822 0.044 Uiso 1 1 calc R
H4B H 0.7112 0.4331 0.2296 0.044 Uiso 1 1 calc R
C5 C 0.4600(8) 0.1881(8) 0.2715(5) 0.0433(17) Uani 1 1 d .
H5A H 0.5001 0.2829 0.3001 0.052 Uiso 1 1 calc R
H5B H 0.3640 0.1525 0.3003 0.052 Uiso 1 1 calc R
C6 C 0.5594(8) -0.0952(8) 0.2444(6) 0.0477(18) Uani 1 1 d .
H6A H 0.5474 -0.1722 0.2684 0.057 Uiso 1 1 calc R
H6B H 0.4834 -0.1212 0.1884 0.057 Uiso 1 1 calc R
C7 C 1.0739(8) 0.2737(8) 0.3012(6) 0.0492(19) Uani 1 1 d .
H7A H 1.1232 0.2614 0.2423 0.059 Uiso 1 1 calc R
H7B H 1.1545 0.2887 0.3531 0.059 Uiso 1 1 calc R
C8 C 0.4203(7) 0.1632(8) 0.1718(5) 0.0395(16) Uani 1 1 d .
H8A H 0.3540 0.0721 0.1454 0.047 Uiso 1 1 calc R
H8B H 0.3609 0.2212 0.1599 0.047 Uiso 1 1 calc R
C9 C 0.8322(9) -0.0602(9) 0.2849(6) 0.055(2) Uani 1 1 d .
H9A H 0.8479 -0.1469 0.2663 0.066 Uiso 1 1 calc R
H9B H 0.7974 -0.0469 0.3481 0.066 Uiso 1 1 calc R
C10 C 0.5238(9) 0.0079(8) 0.3157(5) 0.0463(18) Uani 1 1 d .
H10A H 0.4089 -0.0154 0.3210 0.056 Uiso 1 1 calc R
H10B H 0.5787 0.0178 0.3769 0.056 Uiso 1 1 calc R
C11 C 0.9835(8) 0.0437(8) 0.2840(6) 0.0472(18) Uani 1 1 d .
H11A H 1.0631 0.0504 0.3340 0.057 Uiso 1 1 calc R
H11B H 1.0269 0.0242 0.2236 0.057 Uiso 1 1 calc R
C12 C 1.0106(8) 0.3847(8) 0.3146(6) 0.0492(19) Uani 1 1 d .
H12A H 0.9825 0.4087 0.3788 0.059 Uiso 1 1 calc R
H12B H 1.0906 0.4608 0.3036 0.059 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
O4 Zn1 O1 101.02(19) .
O4 Zn1 O2 98.80(18) .
O1 Zn1 O2 75.38(19) .
O4 Zn1 O5 75.57(17) .
O1 Zn1 O5 90.32(19) .
O2 Zn1 O5 163.5(2) .
O4 Zn1 O3 77.11(18) .
O1 Zn1 O3 148.88(18) .
O2 Zn1 O3 74.27(19) .
O5 Zn1 O3 118.46(18) .
O4 Zn1 Br1 149.91(14) .
O1 Zn1 Br1 106.75(14) .
O2 Zn1 Br1 99.18(14) .
O5 Zn1 Br1 92.73(13) .
O3 Zn1 Br1 84.82(13) .
O6 Zn2 Br2 109.00(12) .
O6 Zn2 Br3 104.31(13) .
Br2 Zn2 Br3 121.63(5) .
O6 Zn2 Br1 97.37(13) .
Br2 Zn2 Br1 110.55(5) .
Br3 Zn2 Br1 110.97(5) .
Br4 Zn3 Br5 114.80(5) .
Br4 Zn3 Br6 112.64(5) .
Br5 Zn3 Br6 110.19(4) .
Br4 Zn3 Br6 111.63(5) 2_646
Br5 Zn3 Br6 111.12(5) 2_646
Br6 Zn3 Br6 94.77(4) 2_646
Zn1 Br1 Zn2 105.04(4) .
Zn3 Br6 Zn3 85.23(4) 2_646
C12 O1 C4 114.3(5) .
C12 O1 Zn1 116.9(4) .
C4 O1 Zn1 128.6(4) .
C7 O2 C11 113.9(5) .
C7 O2 Zn1 110.6(4) .
C11 O2 Zn1 112.6(4) .
C6 O3 C9 112.8(5) .
C6 O3 Zn1 107.7(4) .
C9 O3 Zn1 113.6(5) .
C5 O4 C10 117.3(5) .
C5 O4 Zn1 114.9(4) .
C10 O4 Zn1 117.0(4) .
C8 O5 C3 116.5(5) .
C8 O5 Zn1 113.8(4) .
C3 O5 Zn1 127.9(4) .
C1 O6 C2 114.4(6) .
C1 O6 Zn2 122.9(4) .
C2 O6 Zn2 122.4(4) .
O6 C1 C3 110.1(6) .
O6 C2 C4 111.6(5) .
O5 C3 C1 110.3(5) .
O1 C4 C2 110.5(6) .
O4 C5 C8 110.6(6) .
O3 C6 C10 110.9(6) .
O2 C7 C12 106.6(6) .
O5 C8 C5 107.5(5) .
O3 C9 C11 107.6(6) .
O4 C10 C6 108.7(5) .
O2 C11 C9 105.7(6) .
O1 C12 C7 107.5(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 2.055(4) .
Zn1 O1 2.086(5) .
Zn1 O2 2.114(5) .
Zn1 O5 2.201(5) .
Zn1 O3 2.226(5) .
Zn1 Br1 2.4254(12) .
Zn2 O6 2.080(5) .
Zn2 Br2 2.3054(13) .
Zn2 Br3 2.3196(12) .
Zn2 Br1 2.4586(12) .
Zn3 Br4 2.3208(12) .
Zn3 Br5 2.3665(14) .
Zn3 Br6 2.4666(12) .
Zn3 Br6 2.4861(12) 2_646
Br6 Zn3 2.4861(12) 2_646
Br7 Br8 2.2868(13) .
O1 C12 1.432(8) .
O1 C4 1.454(9) .
O2 C7 1.431(9) .
O2 C11 1.435(10) .
O3 C6 1.419(8) .
O3 C9 1.441(9) .
O4 C5 1.429(8) .
O4 C10 1.464(8) .
O5 C8 1.424(7) .
O5 C3 1.445(7) .
O6 C1 1.442(7) .
O6 C2 1.443(8) .
C1 C3 1.487(10) .
C2 C4 1.486(9) .
C5 C8 1.460(10) .
C6 C10 1.477(11) .
C7 C12 1.477(11) .
C9 C11 1.504(11) .
